Emulsion for the conditioning of raw cotton fibers



United States Patent 3,177,143 EMULSION FOR THE CONDITIONING 0F RAW (IQTTON FIBERS Frederick T. Lense, Mauldin, S.C., assignor to Esso Research and Engineering Company, a corporation of Delaware N0 Drawing. Filed Aug. 29, 1961, Ser. No. 134,568 5 Claims. (Cl. 252--8.9)

This invention relates to the use of branched chain alcohols and emulsions thereof in fiber processing. The invention is applicable to the conditioning of raw cotton, organic derivatives of cellulose, and other fibers having Wettability characteristics equivalent to such fibers, but is especially directed to the conditioning of lint cotton fibers prior to spinning.

This is a continuation-in-part of application Serial Number 815,327, filed May 25, 1959 and application Serial Number 815,322, also filed on May 25, 1959, both now abandoned.

In the processing of such raw textile fiber stock, it has heretofore been customary to apply, as by spray or wiping action, a conditioning fluid, such as a mineral oil or an oil compounded with modifying substances, to the raw fibers, after they have been separated from the raw mat, to facilitate the subsequent operations of forming them into yarn or thread. For example, in the processing of cotton, the bale of raw cotton is usually passed to a bale breaker and cleaner, where the raw mat is formed and dirt and dust are largely removed. The resulting mat is then passed to a picker where a beater roll separates the raw cotton fibers from the mat. The separated fibers are then subjected in series to the usual carding, drawing and roving operations, and finally to spinning to form yarn or thread. The latter then passes to the looms where the weaving operation is carried out to form cloth. The conditioning treatment of the raw fibers by the conditioner fluid application may take place when the bale is opened or at any subsequent step leading to the spinning operation per so as, for instance, at the beater roll of the picker immediately after the fibers have been separated from the mat.

The term spinning in the broad sense refers collectively to all of the operations in manufacturing a yarn from fibrous raw material. The specific operation known as spinning may be defined as the operation of drafting roving to the required counts, inserting the required number of turns per uni-t of length in the yarn, and winding it into the form of a cop or onto a bobbin or spool. Since the specific discussions herein relate to the processing of natural fibers the term spinning is used herein in accordance with the later, more narrow definition. It is to be understood that in the processing of synthetic fiber the term is used to include the extrusion of a spinning solution through spinnerettes to form filaments.

It is the object of such treatment to reduce fly and dust in the carding room, to increase the flexibility and pliability of the fibers for the subsequent operations with a view to producing a higher percentage of long fibers and fewer short or broken fibers, and to reduce the generation of static electricity in the subsequent processing without requiring excessive humidification.

The conditioners having a mineral oil base have not been entirely satisfactory. It has been found that their use in many instances results in an objectionable degradationin tensile strength of the spun yarn. These conditioners have also presented problems of fiber discoloration.

Likewise, the straight chain higher aliphatic alcohols, such as stearyl and oleyl alcohols, leave a solid residue that is objectionable because it is difiicult to remove from the fibers and therefore adversely affects their dyeing characteristics.

It has now been found that a new source of fiber conditioners can be prepared from certain high molecular Weight alcohols.

Therefore, this invention relates in particular to the use of branched chain, C to C particularly C to C and preferably C to C monohydric alcohols which are liquid at room or field temperatures above about 40 F., as lubricants and anti-static agents in the carding, drawing, spinning, twisting, coning, pirning, banking, weaving, knitting and associated mechanical operations of fiber processing. I

One aspect of the invention relates to the use of these alcohols in fiber processing. Another aspect of the invention relates to the use of 25 to wt. percent aqueous emulsions of these alcohols containing an emulsifying agent which does not impart substantial wettability to the emulsion in the carding, drawing, and spinning of cotton fibers.

The preferred emulsion for use in the aforesaid processes are relatively stable aqueous emulsions of the aforedescribed alcohols which may be formed by simple agitation with low concentrations of an emulsifier compound having an organic hydrophobic component and a polyalkylene oxide hydrophilic component wherein the weight relationship between such components is balanced in a manner that will not impart substantial wetting properties to the emulsifier.

It is known that higher molecular weight alcohols are not emulsifiable in or with water unless an emulsifying agent is added,

Providing the wetting properties of the emulsifier are sufficiently low, concentrations of emulsifier may be used in accordance with this invention up to as high as 10 wt. percent based on the weight of water in the emulsion. Obviously, however, much lower concentrations, e.g. 0.05 to 1.0, preferably below 0.2 wt. percent, are preferred, both with regard to cost and with regard to the aforementioned wetting properties; The preferred emulsions may be etfected by simple agitation and remain stable for periods adaptable for diversified .use, e.g. from 1 to 24 hours, and be reformed after de-emulsification in the same manner. Emulsions of the aforedescribed ingredients which will remain stable for much longer periods can be effected by homogenization, colloid milling and ultrasonic devices known to the art. The alcohols or emulsions may be applied to cotton fibers in amounts up to about 10 wt. percent of the said fibers without wetting such fibers to a degree that will deleteriously affect the subsequent use of such fibers in conventional, mechanical textile processing operations. For most purposes it will be found that about 0.2 to 10 wt. percent of the liquid is satisfactory. Even very small amounts, e.g. 0.05 Wt. percent of the fiber, have anoticeable effect. However, applications from about 0.5 to 2.0 wt. percent are preferred.

Suitable alcohols for use in this invention are preferably prepared by the Aldox process, a modification of the Well-known Oxo process.

In the Aldox process, a primary alcohol product is prepared from an olefin and a synthesis gas of carbon monoxide and hydrogen. Except for the use of a reaction modifier hereinafter discussed, and the product, the Alclox process is substantially the same as the 0x0 process. the 0x0 process, oxygenated organic compounds are synthesized in the presence of a cobalt catalyst from organic compounds containing olefinic linkages by reaction with carbon monom'de and hydrogen. In this reaction, predominantly-aldehydes and minor proportions of ketones and alcohols are formed. The products from this OX0 step may then be hydrogenated in a second stepto conbranched alkanols.

vert the organic carbonyl. compounds containing one i more carbon atom than the 'olefinic starting material to the corresponding alcohol. The hydrogenation catalyst may comprise any known reduction catalyst such as metallic supported or unsupported nickel, copper chromite,

sulfactive catalyst such as oxides and sulfides of tungsten, nickel, molybdenum and the like. a

Straight and branched chain olefins such as propylene,

7 carbon synthesis process, thermal or catalytic cracking operations, and other sourcesof hydrocarbon fractions containing such olefins may be used .as starting materials depending on the nature of the final product desired. The synthesis gas mixture fed to the first stage may be any desired ratio of H to CO, preferably within the limit of 0.5 to 2 volumes hydrogenper volume of carbon monoxide. The conditions for reacting olefins with the synthesis gases vary somewhat in accordance with the nature of the olefin feed, the reaction being generally conducted at pressures in the range of from about 1500 to .4500 p.s.i.g.' and the ratio of synthesis gas 'to olefin may vary widely; in general about 2500 to 25,000 cubic feet of employed in the form of an -oilsoluble compound of the,

catalytically active carbonylat-ion metal. Thus, there have i been employed the salts .of the metals such as cobalt and a high molecular weight fatty acid such as stearic, oleic, naphthenic, linoleic. and the like. Water-soluble catalyst, such as cobalt acetate, chloride, and the like, may also be used. Catalyst concentrations may vary from about 0.05 to 1.0% by weight of the catalyst calculated as cobalt on olefinic feed. The first stage for carbonyla tion reaction may be carried out at temperatures in the range of from about 250 to 450 F. depending upon the nature of the olefin and other reaction conditions. In general, the lower olefins will react at lower temperatures and will react to a greater extent than the highermolecular weight olefins.

'The Oxo process without modification will produce some alcohols of higher molecular weight, but theyields of such products are relatively low. These alcohols result from several difierent mechanisms including aldolization, dehydration, dirnerization', 'acetalization; etc. Some of these alcohols contain two more than twice the number of carbons in the olefin feed and are highly Another type contains three morev d r 7 described may also be produced in the Aldox process in some-what lesser quantities. The C to;C alcohols of this groupmay alsobe 'used in this invention. j

A liquid oxygenated reaction product comprising alde hydes-frorn the corbonylation reaction containing inorganic contaminants, e.g.'"dissolved cobalt carbonyl-and Zinc salts, is sen-t to a catalyst decomposition or decobalting zone, where in the presence of heat and steam,'water,

. ventional conditionsto alcohols "and the alcohol product than twice the number of carbons in the olefin "feed but 7 this latter type also contains an additional oxygen atomf in the molecule forming an etherlinkage with two inter-,-

nal carbon atoms.

Fora more detailed description of these ether'alcohols see Oxo Ether Alcohols, Bartlett et at, Industrial and Engineering Chemistry, March 1959, pages 257- In the Aldox process the same reactors, catalyst, and

reaction conditions may be employed as in the 'aforedescribed Oxo process, and, in additio'n, a reaction-modifier is employed which' results. in the production, .in high yields, of a primary alcohol product having 2n+2 carbon fatty acids, oxides, hydroxides, carbonates, and also metallic salts of cobalt hydrocarbonyl. Thus, in the Aldox process 'there is passed into thefirst-stage reaction zone.

along with the olefin .carbon monoxide,'hydrogen, and cobaltcarbonylation catalyst, a reaction modifier, preferrably zinc; Other Aldox'modificrs havebeen suggested in the prior art. V g I, The mono-ether,- mono-hydroxy alcohols herein-before fractionated to produceboth the n+1 and2n'+2 alcohols,

as described.

The production of such alcoholsl'by the Aldox process is covered by US, Patent 2,811,567. r

Monohydric, primary alcohols may also be prepared from aldehydes via conventional Aldol condensation. By this process the positive end of a carbonyl group is linked with a carbanion by a typical ald-olcondensation known to the art- The primary .Aldol product may then be dehydrated by means known to the art toyield an unsaturated aldehyde -which can. be hydrogenatedto a primary alcohol.

Another'method for preparing monohydric, primary alcohols is by the process-known to theart as the Guerbet reaction. 7 V

Particularly suitable emulsifiers for usewith-this invention are those havinga hydrocarbon comprising hydrophobic group containing 20-60, preferably 20-36, carbon atoms and apolyalkylene oxide hydrophilic group which emulsifiers of this type arefsoldcommercially and may be prepared by various methodswell known to the art.

A particularly good emulsifier for this purpose is marketed under the trade name of lgepal DM-880.' The alkylene oxide units in thehydrophilic group may be either ethylene oxide or propylene oxide with the former preferred. Of

these, the most preferred are dialkyl phenoxy polyoxy ethylene ethanol, type non-ionic emulsifiers wherein the alkyl substituents" of the phenol nucleus contain at least '9 carbon :atoms each and the. ethylene oxide units con1 prise -95 wt. percent ofthe compound. .With the most preferred-type of emulsifierujust described, the emulsions of thisinven'tion may beefiected with emulsifier concentrations in the, range of .005 to 0.2%, preferably 0.075 vto 0.125%, based on'the weight of water in theemulsion. Such emulsifiers have the added .advantage thatthey'may be used with the alcoholsof this invention in much larger quantities, i.e.,,above 1%, if desired, Without producing a noticeable increase in the wetting properties. 7 j] Another variationof this type of emulsifier which does 9 not impart substantialwettability to the alcohols of this invention may also be prepared-whereinthe hydrophobic element is a polyoxyalkylene, e.g. polyoxypropylene, polymer prepared by the ,condensation ofpropylene oxide, or a .higher; alkylene. oxide, e.g.lbut-ylen e oxide,

with an organic base compound containing at. least-one and preferablyafpluralit'y of reactive. hydrogen atoms, e.g. propylene glycol, monofunctionalalcohols'.such as butanol, secondaryamines such as diethyl amine, etc, and

the hydrophilicgroup deformed by-condensing ethylene oxidewith the aforesaid hydrophobic element'. T

in U.S.'-,Patents -2,67'4,619:and 2,677,700, and elsewhere in the literature. (l950), vol.' 26,;llo. l0,. beg'inning'at page tt); The

- Journal of the American Oil Chemists Society (1951), 75

vol. 28, bcginninggat page 294; and-vol. 29 :(1952), of

Emulsifiersof this, general type are discussed in detail See Soap 5 and Sanitary Chemicals the same publication beginning at page 240. These emulsifiers may be tailored to specific uses by controlling the hydrophobic-hydrophilic balance and the molecular weight of both the hydrophobic and hydrophilic groups.

Thus, the advantages to be gained by emulsifying water and higher molecular weight alcohols such as hereinbefore described with the emulsifiers described herein are at least twofold. First, an emulsifier is employed which adds little or nothing to the wetting properties of the alcohol and water per se and, second, stable emulsions can be effected with extremely low concentrations of the emulsifier thereby minimizing any potential increase in wetting properties. Neither water nor higher molecular weight alcohols such as those hereinbefore described will wet out cotton fibers under ordinary conditions of temperature and pressure when applied in the range of to 10 wt. percent based on the weight of cotton fibers.

A convenient reference which may be used to characterize an emulsifier that will impart substantial wettability to the emulsions is provided by identifying the undesirable emulsifier as one that will reduce the wetting time of a C branched chain, monohydric, primary alcohol-water emulsion below about 15 minutes as meas ured by Standard Test Method 17-1952 set forth in the 1958 Technical Manual of the American Association of Textile Chemists and Colorists at page 152 using standard test skeins of 2-ply cotton yarn, 0.1 wt. percent emulsifier based on weight of water, and a 25/75 water to alcohol weight ratio.

The term branched chain, monohydric, primary alcohol as used herein shall be construed to include both monohydric, primary alcohols which aside from the hydroxyl group are composed exclusively of carbon and hydrogen atoms and monohydric, primary alcohols which aside from the hydroxyl group are composed of carbon atoms, hydrogen atoms and a single oxygen atom forming an ether linkage with two of such carbon atoms.

Example I A branch chain C monohydn'c alcohol wherein the carbinol group is positioned intermediate to the ends of the longest carbon chain was prepared by the Aldox process. This process and the range of operating conditions within which it may be carried out had previously been discussed herein. The alcohol of this example was prepared by this process employing as the olefin feed a C olefin fraction previously prepared by a U.O.P. type polymerization of a C to C olefin stream, cobalt and zinc catalyst in the form of their oil-soluble fatty acid salts, i.e. oleates, and under the following operating conditions.

Carbonylation reaction: C olefin feed rate Catalyst concentration l0-530 b./d. .08 wt. percent cobalt (on olefin), .02 wt. percent zinc (on olefin). Temperature, F. 350-360. Pressure, p.s.i.g. 3000-3500.

Ratio of H to CO in synthesis gas mixture 1:1.421.

1 Barrels per day.

'A 25/75 wt. percent of water/ alcohol was preparedby blending the C alcohol prepared above with water and 0.1 wt. percent based on said water, of a commercially available non-ionic emulsifying agent comprising a dinonyl phenol alkylene oxide condensate containing about to wt. percent ethylene oxide per molecule.

In a textile spinning mill where raw bale cotton is blended, sprayed with a fiber lubricant, matted, carded into rovings, and then spun into yarn and threads, tests were conducted with the above-described alcohol emulsions. Other tests were conducted using a commercially available fiber lubricant having a hydrocarbon base. The latter lubricant was being used for this purpose by the mill at the time the tests were conducted.

In each test the lubricant was placed in a storage tank from which it was fed by separate proportioning pumps into spray nozzles attached to fine cotton openers. Each opener handles about lbs/hr. of raw baled cotton. About 0.5 to 0.75 wt. percent of lubricant was added in each test. The lubricated cotton was then blended, mat rolled, transferred to the carding machines and subsequently spun into yarn. A major proportion of the trash included with the lint cotton is removed at the carding step.

With regard to the cotton sprayed with the aforesaid alcohol emulsion, the following observations were made.

(1) No problems resulting from a build-up of static electricity were detected.

(2) The appearance of the alcohol sprayed cotton with relation to cleanliness was improved, indicating more trash removal.

(3) The alcohol sprayed cotton demonstrated a luster not evident with that sprayed with hydrocarbon comprising lubricant.

(4) The alcohol sprayed cotton demonstrated a better evenness in the yarn and fewer slubs in the card web. The average reduction in these when compared to the cotton sprayed with the hydrocarbon comprising lubricant was in the order from 9 to 6, an improvement of roughly 50% The term sub as used herein refers to a soft, thick uneven place in a yarn.

Example II Cotton is sprayed with an emulsion prepared as in Example I from a C branched chain, monohydric, primary alcohol made in accordance with the method described in the aforementioned example while using a C olefin feed. The cotton is blended, mat rolled, carded and subseqeuntly spun into yarn and thread. The results are comparable to those obtained in Example I.

Example III Cotton is sprayed, as described in Example I, with a C branched chain, monohydric, primary alcohol prepared in accordance with Example I. The cotton is blended, mat rolled, carded and subsequently spun into yarn and thread. The results are comparable to those obtained with the emulsion in the aforemetnioned example.

Example IV Cotton is sprayed, as described in Example I, with a C branched chain, monohydric, primary alcohol prepared in accordance with Example I. The cotton is blended, mat rolled, carded and subsequently spun into yarn and thread. The results are comparable to those obtained with the emulsion in the aforementioned example.

What is claimed is:

1. An emulsion consisting essentially of 25 to 75 Wt. percent of a C to C branched chain, monohydric, primary alcohol containing 25 to 75 wt. percent water and 0.05 to 10 wt. percent, based on said water, of a nonionic emulsifying agent containing a hydrophobic group consisting of a dialkyl substituted phenol containing 20 to 36 carbon atoms wherein each alkyl substituent contains at least 9 carbon atoms and a polyalkylene oxide 7 g r V hydrophilic group comprising 70 to 95 Wt. percent of said said emulsifying agent is a dinonyl phenol ethylene oxide agent, wherein said alcohol is a liquid at temperatures" condensate.

between 40? and 115 F.

2. An emulsion in accordance with claim 1 wherein I Referencescitedby the Examiner said polyalkylene oxide is a polyethyleneoxide condensate.' 5 UNITED STATES PATENTS v 3. An emulsion in accordance With claim 1 wherein 2,054,257 97/36 H'ueter 252 ;312 XR said polyalkylene oxide comprises between 85 and 95 Wt. 2 132 3 10 3 Bel-Sch percent of said agent. I o i 2,150,568 3/39 Whitehead.

4. An. emulsion in accordance with claim 1 wherein 2,677,700 5/54 Ja kson et al 250 488 said emulsion contains 0.075 to 0.125 Wt. percent of said 10 T a a e emulsifying agent'basedon the weight of said Water. WJLLLIAM MARTIN Pnmary Examiner 5. An. emulsion .in accordance with claiml wherein RICHARD D. NEVIUS, Examiner. 

1. AN EMULSION CONSISTING ESSENTIALLY OF 25 TO 75 WT. PERCENT OF A C16 TO C20 BRANCHED CHAIN, MONOHYDRIC, PRI MARY ALCOHOL CONTAINING 2K TO 75 WT. PERCENT WATER AND 0.05 TO 10 WT. PERCENT, BASED ON SAID WATER, OF A NONIONIC EMULSIFYING AGENT CONTAINING A HYDROPHOBIC GROUP CONSISTING OF A DIALKYL SUBSTITUTED PHENOL CONTAINING 20 TO 36 CARBON ATOMS WHEREIN EACH ALKYL SUBSTITUENT CONTAINS AT LEAST 9 CARBON ATOMS AND A POLYALKYLENE OXIDE HYDROPHILLIC GROUP COMPRISING 70 TO 95 WT. PERCENT OF SAID AGENT, WHEREIN SAID ALCOHOL IS A LIQUID AT TEMPERATURES BETWEEN 10* AND 115*F. 